HRID1994346

反应详情

EQUATION

反应方程式

HRID 1994346 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

3

PROCEDURE

实验过程

Trityl chloride (9.43 g) is added in one portion to a solution of 2-hydroxymethyl-5-methoxy-4-pyridone (5 g) and 4-dimethylaminopyridine (4.2 g) in dry dimethylformamide (80 mL) and the solution stirred at room temperature for 12 hours. The mixture is then heated on a steam bath for 3 hours and diluted with iced water (300 mL) to give a light brown solid. The solid is collected, washed with water and sucked dry. The solid is dissolved in hot ethyl acetate to give a clear solution which immediately deposits a granular off-white solid. The solid does not redissolve on further heating. After cooling the solid is collected, washed with ethyl acetate and diethyl ether and dried to give 5-methoxy-2-trityloxymethyl-4-pyridone (7.5 g) as an off-white solid, m.p. 185-7° C.

WORKUP

后处理

  1. temperatureThe mixture is then heated on a steam bath for 3 hours
  2. customto give a light brown solid
  3. customThe solid is collected
  4. washwashed with water
  5. customsucked dry
  6. dissolutionThe solid is dissolved in hot ethyl acetate
  7. customto give a clear solution which
  8. dissolutionThe solid does not redissolve on further heating
  9. temperatureAfter cooling the solid
  10. customis collected
  11. washwashed with ethyl acetate and diethyl ether
  12. customdried